STRUCTURAL AND SOLID-STATE P-31 NMR-STUDIES ON A NOVEL FLUOROTRIS(TRIPHENYL-PHOSPHINE)COPPER(I) ADDUCT

The synthesis of the title compound as its triphenylphosphine/methanol solvate, [(PPh3)3CuF].4PPh3.4MeOH, is reported together with characterization by solid-state P-31 CP-MAS n.m.r. and single-crystal X-ray diffraction. Crystals are trigonal, space group P3, with a 14.453(5), c 15.388(6) angstrom. The structure refined to a final R value of 0.049 for 1926 'observed' [I > 3-sigma-(I)] reflections. The (PPh3)3CuF molecule lies on a crystallographic threefold axis. Cu-F is 2.115(9) angstrom, and Cu-P 2.323(3) angstrom. The solid-state P-31 n.m.r. spectrum is dominated by peaks from each of the four solvated PPh3 molecules at -1.6, -5.4, -10.6 and -14.2 ppm with respect to 85% H3PO4. The quartet of lines arising from the ligands coordinated to the copper atom shows an average chemical shift of -5 ppm and approximately equal line spacings of 1.0 kHz.